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Preparation of hollow nanosilica white sphere

A nano-silica, hollow technology, applied in the direction of silicon oxide, silicon dioxide, etc., can solve the problems of time-consuming, complicated preparation process, and difficulty in obtaining hollow nano-silica balls, and achieve low energy consumption, simple operation, and high synthesis conditions mild effect

Inactive Publication Date: 2010-10-27
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Overcome the complex and time-consuming preparation process in the prior art, and it is difficult to obtain hollow nano-silica spheres with particles smaller than 100nm

Method used

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  • Preparation of hollow nanosilica white sphere
  • Preparation of hollow nanosilica white sphere
  • Preparation of hollow nanosilica white sphere

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preparation example Construction

[0032] A preparation method of hollow nano-silica spheres, the specific preparation steps are as follows:

[0033] 1) Dissolving the structure directing agent, water and inorganic electrolytes of different concentrations to form a clear solution I;

[0034] 2) Add the silicon source precursor to solution I under vigorous stirring, stir the mixture at 12-40°C for 10-48 hours, transfer the mixture into a reaction kettle, and conduct hydrothermal crystallization at 60-120°C for 24-48 hours;

[0035] 3) The product is filtered and washed with water until the filtrate is clarified and then dried at room temperature;

[0036] 4. The structure-directing agent of the obtained product was extracted with a mixed solution of ethanol and HCl at 60-70° C. for 6 hours. Add 200 mL of ethanol and 2 g of concentrated hydrochloric acid to 1 g of the product to obtain the product of the present invention.

Embodiment 1

[0038] Under stirring at 20°C, dissolve 0.8g of F127 in 28mL of 0.04M NaH 2 PO 4 -Na 2 HPO 4 Buffer solution (pH=6.86), after the solution is clarified, add 2.7g (MeO) 3 SiCH 2 CH 2 Si(OMe) 3 , and aged at 20°C for 24h with stirring. The obtained mother liquor was transferred to the reactor for crystallization at 100°C for 24h. After the product was filtered, washed with water and dried, it was extracted with a mixed solution of absolute ethanol and HCl at 70°C for 24 hours. After the product was filtered and dried, a white lumpy light solid was obtained.

[0039] Respectively using FEI Tecnai G 2 Spirit transmission electron microscope (TEM) and ASAP2020 specific surface analyzer of Mike Company of the United States were used to characterize the samples.

[0040] figure 1 The transmission electron microscope (TEM) photo of the product obtained in the present embodiment 1 is provided; TEM result shows that the product obtained is a hollow nanosphere with uniform pa...

Embodiment 2

[0042] Adopt the preparation process of embodiment 1, its difference is that, add 1.08g (MeO) 3 SiCH 2 CH 2 Si(OMe) 3 as a silicon source. A white lumpy light solid was obtained. The representation method is the same as above. TEM results show that the obtained product is a hollow nanosphere with uniform particle size and good dispersion; the size of the hollow nanosphere is 15nm, the inner diameter is 8nm, and the wall thickness is 7nm. The BET specific surface area of ​​the material is 969m 2 g -1 ; Pore volume is 2.91cm 3 g -1 .

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Abstract

The invention relates to a silicon oxide sphere particle, in particular to a method for preparing a hollow nano silicon oxide sphere. In a bionic system with room temperature approximately neutral, the three block copolymer F1127 is taken as a structure guiding agent, the mutual interactions between hydrolytic oil-soluble silica resources and the three block copolymer F1127 and inorganic electrolytes are controlled, the hollow spherical particle is obtained by steps of the preparation of polymer micelle, hydrolytic polymerization of silica resources, hydrothermal crystallization, drying and extraction of the structure guiding agent; the size of the spherical particle is continuously adjusted in the range of between 10 and 20nm, and the thickness of a shell wall is continuously adjusted inthe range of between 4 and 10nm. The synthesized nano hollow sphere has the advantages of big specific surface, big hole capacity, uniform particle size and good dispersibility of the particle, a multi-level structure formed between nano hollow spheres and high mechanical stability and thermal stability, etc.

Description

technical field [0001] The invention relates to silica sphere particles, in particular to a method for preparing hollow nanometer silica spheres. Background technique [0002] Nanomaterials with hollow structures are currently a hot topic in the field of material research. The polymer micelle can be used to form a polymer hollow structure with a particle size of 1-100 nm. However, most polymer hollow spheres are unstable and swell in air, which severely limits their practical application. Inorganic hollow nanospheres with a particle size between 1 and 100 nm are functional materials with a special structure. Due to their large specific surface area, high storage capacity, and good mechanical and thermal stability, they have attracted widespread attention in the field of nanotechnology. , It has broad application prospects in the research fields of nano-confinement catalysis, targeted drug (gene) release, adsorption, artificial cells, insulating materials, photonic crystals...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/113C01B33/18
Inventor 杨启华刘健李灿张磊
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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